Methylamine → methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate

HRID 59734

반응식

HRID 59734 반응식
Cl[S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3].C1COCC1.[CH3:19][NH2:20]>C(Cl)Cl>[CH3:19][NH:20][S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3]

참가 물질

5

반응물 3

HCID 6329MethylamineHCID 8028TetrahydrofuranHCID 27367332-Thiophenecarboxylic acid, 3-(chlorosulfonyl)-, methyl ester

생성물 1

HCID 12906749methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of methyl 3-(chlorosulfonyl)thiophene-2-carboxylate (500 mg, 2.077 mmol) in DCM (20 ml), methanamine 2N solution in THF (4.155 ml, 8.31 mmol) was added and the reaction was stirred for 1 hour at RT. The mixture was partitioned between 2N HCl and DCM and the aqueous phase was extracted with DCM. The combined organic layers were dried over sodium sulfate and the solvent was removed affording methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate (Int. 32) (430 mg, 1.828 mmol, MS/ESI+235.8 [MH]+).

후처리

  1. customThe mixture was partitioned between 2N HCl and DCM
  2. extractionthe aqueous phase was extracted with DCM
  3. dry with materialThe combined organic layers were dried over sodium sulfate
  4. customthe solvent was removed

출처 및 근거

ORD 기록
ord-9b66d920a79c456da03aea4e17f10758
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440954B2

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